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Preparation method of immobilized ionic liquid used for ester exchange reaction

A technology of transesterification reaction and ionic liquid, which is applied in the preparation of organic carbonate, chemical instruments and methods, organic chemistry, etc., can solve the problems of difficult catalyst recovery and high cost, achieve good immobilization effect, reduce preparation cost, and improve catalytic activity high effect

Active Publication Date: 2014-12-24
灯塔森佳新能源合伙企业(有限合伙)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The technical problem to be solved in the present invention is to aim at the defects such as difficulty in catalyst recovery and high cost in the transesterification reaction of current ionic liquid catalysts.

Method used

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  • Preparation method of immobilized ionic liquid used for ester exchange reaction
  • Preparation method of immobilized ionic liquid used for ester exchange reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] In the round bottom flask, add toluene, pure silicon molecular sieve MCM-41, epichlorohydrin and zinc chloride successively, wherein the mass ratio of pure silicon molecular sieve MCM-41 to toluene is 1:20, pure silicon molecular sieve MCM-41 and ring The mass ratio of oxychloropropane is 10:1, and the amount of zinc chloride is 2% of the mass of pure silicon molecular sieve MCM-41. The reaction was carried out under magnetic stirring at 80° C. for 6 hours to obtain a pure silicon molecular sieve whose surface hydroxyl groups were etherified.

[0023] Put the solid obtained in the above process into a round-bottomed flask, wash and dry it, then put it into a dry round-bottomed flask, and then add toluene and 1-methylimidazole in sequence, wherein the mass ratio of toluene to solid is 10:1, 1 - The mass ratio of methylimidazole to solid is 1:1, and heated to 80°C for 6 hours with magnetic stirring to obtain an immobilized ionic liquid catalyst supported by pure silicon m...

Embodiment 2

[0025] In the round bottom flask, add toluene, pure silicon molecular sieve MCM-48, epibromohydrin and ferric chloride successively, wherein the mass ratio of pure silicon molecular sieve MCM-48 to toluene is 1:50, pure silicon molecular sieve MCM-48 and ring The mass ratio of oxybromopropane is 5:1, and the amount of ferric chloride is 2% of the mass of pure silicon molecular sieve MCM-48. The reaction was carried out under magnetic stirring at 80° C. for 6 hours to obtain a pure silicon molecular sieve whose surface hydroxyl groups were etherified.

[0026] Put the solid obtained in the above process into a round bottom flask, wash and dry it, then put it into a dry round bottom flask, then add toluene and 1-ethylimidazole in sequence, wherein the mass ratio of toluene to solid is 10:1, 1 -The mass ratio of ethylimidazole to solid is 2:1, and heated to 80°C for 6 hours with magnetic stirring to obtain an immobilized ionic liquid catalyst supported by pure silicon molecular s...

Embodiment 3

[0028] Add toluene, pure silicon molecular sieve SBA-15, epibromohydrin and ferric chloride in turn in the round bottom flask, wherein the mass ratio of pure silicon molecular sieve SBA-15 to toluene is 1:30, pure silicon molecular sieve SBA-15 and ring The mass ratio of oxybromopropane is 6:1, and the amount of ferric chloride is 2% of the mass of pure silicon molecular sieve SBA-15. The reaction was carried out under magnetic stirring at 80° C. for 6 hours to obtain a pure silicon molecular sieve whose surface hydroxyl groups were etherified.

[0029] Put the solid obtained in the above process into a round-bottomed flask, wash and dry it, then put it into a dry round-bottomed flask, then add toluene and 1-propylimidazole in sequence, wherein the mass ratio of toluene to solid is 10:1, 1 - The mass ratio of propylimidazole to solid is 1:1, and heated to 80°C for 6 hours with magnetic stirring to obtain an immobilized ionic liquid catalyst supported by pure silicon molecular ...

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Abstract

The invention relates to a preparation method of an immobilized ionic liquid used for an ester exchange reaction. The preparation method comprises the steps of: regarding a pure silicon molecular sieve as a carrier and regarding epoxy chloropropane or epoxy bromopropane and 1-alkyl imidazole as raw materials to realize efficient immobilization of the ionic liquid on the surface of the pure silicon molecular sieve through two-step reaction. The preparation method is simple; and the obtained immobilized ionic liquid catalyst after the reaction can be recycled for the continuous cyclic utilization through a simple treatment, has a long service life and no pollution, and greatly reduces the reaction cost. Very good catalysis effects can be obtained when the catalyst prepared by the preparation method is used for the ester exchange reaction, such as the ester exchange reaction of dimethyl carbonate and diethyl carbonate and the ester exchange reaction of ethylene carbonate and methanol.

Description

technical field [0001] The invention relates to the field of preparation of immobilized ionic liquids, in particular to a preparation method of an immobilized ionic liquid catalyst used for transesterification. Background technique [0002] At present, most of the catalysts used in the transesterification reaction are alkaline, such as NaOH, KOH, NaOCH 3 、KOCH 3 etc., these catalysts have high activity, but in the actual application process, it is found that this type of catalyst has poor solubility in the reaction solution, is easy to precipitate, and is easy to foul. Precipitation in the medium, clogging the pipeline. Moreover, these catalysts are difficult to separate from the product, which prompts people to study highly active and easy-to-separate heterogeneous catalysts. [0003] Several heterogeneous catalysts have been reported in the literature, such as quaternary ammonium type strong base resin, sulfonic acid type strong acid resin, carboxylic acid type weak aci...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/02C07C68/06C07C69/96
Inventor 薛冰李永昕许杰宁志文李寒羿
Owner 灯塔森佳新能源合伙企业(有限合伙)
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